反应详情

36b (0.38 g, 1.1 mmol) was dissolved in 6 mL of anhydrous CH2Cl2. Triethylamine (1.5 mL) was added followed by 2-cyanoethyl diisopropylchlorophosphoramidite (0.29 mL, 1.3 mmol). The solution was kept at room temperature for 30 min, MeOH (0.1 mL) was added and the reaction was concentrated under vacuum. The residue obtained was partitioned between ethyl acetate and NaHCO3. The organic phase was washed with saturated NaCl, dried over Na2SO4 and concentrated to afford the crude amidite. It was dissolved in 2 mL of ether and added dropwise to ˜50 mL of hexane. The resultant orange solid was collected by filtration, washed with hexane and dried. The yield was 0.4 g.

1. concentrationthe reaction was concentrated under vacuum
2. customThe residue obtained
3. customwas partitioned between ethyl acetate and NaHCO3
4. washThe organic phase was washed with saturated NaCl
5. dry with materialdried over Na2SO4
6. concentrationconcentrated
7. customto afford the crude amidite
8. filtrationThe resultant orange solid was collected by filtration
9. washwashed with hexane
10. customdried